NiFe2O4/C nanocomposites were prepared using the two-step process, including reverse microemulsion followed by thermochemical vapour deposition (TCVD). Micelles made in the first step worked well and NiFe2O4 nanoparticles owing sizes smaller than 10 nanometer with narrow size distribution were obtained. Acetylene gas was used as a carbon source for deposition on the surface of NiFe2O4 nanoparticles. Coating applied for 1 and 2 h at 700°C and resulted in an enhancement of NiFe2O4 nanoparticle size to a level of 30 nanometer. Powder X-ray diffraction (PXRD) patterns revealed the spiel formation for all samples; however, the crystallinity of them has been increased as much as temperature rose to a level of coating. Fourier transform infrared spectroscopy (FT-IR) verified the metal-oxygen bonding linked to the octahedral and tetrahedral vibrations. Micro-Raman spectra for the coated samples were recorded as well, and the results confirmed the existence of ordered and disordered carbon-based materials in nanocomposites. It is noteworthy to mention that, in the sample with 2 h coating time, the defect densities were lower than the sample with an hour coating time. The vibration sample magnetometer (VSM) was also used to investigate the magnetic properties. The as-prepared sample behaves like a superparamagnetic matter; however, the coated ones behave like ferromagnetic materials. The saturation magnetization and coercivity of coated samples were lower than their bulk counterparts which was due to their smaller size.